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High-yield preparation method of small-particle-size functional polymer nanospheres

A technology of nano-microspheres and polymers, which is applied in the field of high-yield preparation of small-diameter functional polymer nano-microspheres, which can solve the problems of reduced polymerization efficiency, low monomer concentration, and large size, and achieve improved curative effect and high The effect of test accuracy

Active Publication Date: 2017-12-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the first type of method, the suspension polymerization system is usually used to prepare large-sized polymer microspheres of 0.01-5mm, and the size of the microspheres prepared by the dispersion polymerization system is usually micron, although the emulsion polymerization system can prepare particles with a particle size of 50-500nm Small particle size microspheres, but the system needs to add stabilizers (emulsifiers), resulting in complicated post-treatment processes, and have a certain impact on the physical and chemical properties of polymer microspheres
The second type of method is generally used to prepare microspheres above 500nm. The monomer concentration of the system is low, which greatly reduces the polymerization efficiency. Acetonitrile and other toxic solvents are often used as the dispersion medium, which is easy to cause environmental pollution and safety problems; distillation, precipitation and polymerization operations Complex, cross-linked precipitation polymerization system is prone to produce irregularly shaped particles and widened particle size distribution after adding the necessary cross-linking agent
The self-stabilizing precipitation polymerization has the characteristics that the particle size of the microsphere increases with the prolongation of the reaction time (the increase of the monomer conversion rate), so although the size of the nucleation is small, such as 100-200nm, at the end of the polymerization, the The prepared polymer microspheres are large in size, usually 0.5-2 μm, and it is difficult to prepare functional polymer nanospheres with small particle size in high yield

Method used

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  • High-yield preparation method of small-particle-size functional polymer nanospheres

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Example 1: Dissolve 1.04g of St and 0.98g of MAH in 50mL of isoamyl acetate, dissolve 0.007g of initiator ABVN in the above solution, pass nitrogen gas for 15min to remove oxygen in the system, and then heat the solution to 45°C Under the reaction 8h. After the reaction was completed, the reaction product was centrifuged at a speed of 4000 r / min for 10 min, and wasoamyl acetate and petroleum ether were added to wash and centrifuge three times. Vacuum-dried to constant weight to obtain functional copolymer nanospheres.

[0046] The yield calculated by gravimetric method is 74%, the microsphere particle size is about 184nm, and the particle size distribution coefficient is 1.03.

Embodiment 2

[0047] Example 2: Dissolve 1.04g of St and 0.98g of MAH in 50mL of isoamyl acetate, dissolve 0.009g of initiator ABVN in the above solution, pass nitrogen gas for 15min to remove oxygen in the system, and then heat the solution to 50°C Under the reaction 8h. After the reaction was completed, the reaction product was centrifuged at a speed of 4000 r / min for 10 min, and wasoamyl acetate and petroleum ether were added to wash and centrifuge three times. Vacuum-dried to constant weight to obtain functional copolymer nanospheres.

[0048] The yield calculated by the gravimetric method is 94%, the particle size of the microsphere is about 267nm, and the particle size distribution coefficient is 1.02.

Embodiment 3

[0049] Example 3: Dissolve 1.04g of St and 0.98g of MAH in 50mL of isoamyl acetate, dissolve 0.007g of initiator ABVN in the above solution, pass nitrogen gas for 15min to remove oxygen in the system, and then heat the solution to 60°C Under the reaction 8h. After the reaction was completed, the reaction product was centrifuged at a speed of 4000 r / min for 10 min, and wasoamyl acetate and petroleum ether were added to wash and centrifuge three times. Vacuum-dried to constant weight to obtain functional copolymer nanospheres.

[0050] The yield calculated by the gravimetric method is 94%, the microsphere particle size is about 278nm, and the particle size distribution coefficient is 1.02.

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Abstract

The invention provides a high-yield preparation method of small-particle-size functional polymer nanospheres. The method adopts a self-stabilization precipitation polymerization manner and is used for polymerizing a charge transfer complex system consisting electron donor monomers and electron receptor monomers to realize high-yield preparation of the small-particle-size functional polymer nanospheres; functional crosslinked polymer microspheres can be prepared by introducing crosslinking monomers into the system, the particle size of the prepared polymer microspheres can be further reduced, and the yield can be increased; small-particle-size core-shell and hollow structure functional microspheres can be further prepared with small-particle-size polymer microspheres as templates. The method has a simple synthesis route and is safe and convenient to operate, the small-particle-size functional polymer nanospheres as well as polymer nanospheres adopting core-shell and hollow structures and other special structures can be prepared with high yield, and the prepared polymer microspheres are uniform in particle size, high in functional group content and applicable to industrial production of the functional polymer nnaospheres.

Description

technical field [0001] The invention relates to a new method for preparing functional polymer nanospheres with high yield through a self-stabilizing precipitation polymerization system, which can be used for the charge transfer complex system composed of electron-donating monomers and electron-accepting monomers Self-stabilizing precipitation polymerization for high yield preparation of functional polymer nanospheres with small particle size. Background technique [0002] Since 1955, the Institute of Emulsion Polymer of Lehigh University in the United States successfully prepared polystyrene microspheres with highly uniform particle size for the first time (Bradford E B, Vanderhoff J W. Electron microscopy of monodisperse latexes [J]. Journal of Applied Physics, 1955, 26 (7):864-871.), the preparation of functional polymer microspheres has become one of the hot spots in the field of polymer research. Monodisperse polymer microspheres have the characteristics of large specif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F222/08C08F2/06C08F218/08C08F222/04C08F222/40C08F222/06C08F257/02C08F222/14C08F212/36
CPCC08F2/06C08F212/08C08F222/04C08F222/06C08F222/40C08F257/02C08F218/08C08F222/08C08F222/102
Inventor 杨万泰孙乔乔陈冬周良宇王力赵长稳马育红
Owner BEIJING UNIV OF CHEM TECH
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